WO2021000458A1 - Procédé de préparation d'oxyde composite de silicium de cérium et produit ainsi qu'application associés - Google Patents
Procédé de préparation d'oxyde composite de silicium de cérium et produit ainsi qu'application associés Download PDFInfo
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- WO2021000458A1 WO2021000458A1 PCT/CN2019/112305 CN2019112305W WO2021000458A1 WO 2021000458 A1 WO2021000458 A1 WO 2021000458A1 CN 2019112305 W CN2019112305 W CN 2019112305W WO 2021000458 A1 WO2021000458 A1 WO 2021000458A1
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- Prior art keywords
- composite oxide
- cerium
- silicon composite
- preparing
- ammonium nitrate
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- RBZGEUJLKTVORU-UHFFFAOYSA-N 12014-84-5 Chemical compound [Ce]#[Si] RBZGEUJLKTVORU-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 26
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000003546 flue gas Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011593 sulfur Substances 0.000 abstract description 12
- 229910052717 sulfur Inorganic materials 0.000 abstract description 12
- 231100000572 poisoning Toxicity 0.000 abstract description 8
- 230000000607 poisoning effect Effects 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract 2
- 238000003483 aging Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 238000001069 Raman spectroscopy Methods 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- -1 cerium ammonium nitrate ethanol Chemical compound 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/20—Reductants
- B01D2251/206—Ammonium compounds
- B01D2251/2062—Ammonia
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Definitions
- the invention belongs to the field of flue gas denitration catalysts, and specifically relates to a preparation method of a cerium-silicon composite oxide and its products and applications.
- the most mature commercial catalyst used to catalyze the NH 3 -SCR reaction is the V 2 O 5 -WO 3 (MoO 3 )/TiO 2 catalyst.
- the catalyst has good activity in the middle and high temperature section (300-400°C).
- its N 2 selectivity is poor in the middle and high temperature section, and its activity in the low temperature section is not ideal.
- V 2 O 5 is also biologically toxic.
- CeO 2 has a special octahedral configuration, which is easy to produce oxygen defects in the crystal, so it has good redox ability. And Ce, as the rare earth element with the largest reserves, is relatively cheap. CeO 2 has been used as an auxiliary, carrier or active component in the NH 3 -SCR field, but the surface of pure CeO 2 is weaker and has a smaller specific surface area. Incorporating SiO 2 into Ce/TiO 2 or V/TiO 2 can effectively increase the acid sites of the catalyst, increase the specific surface area of the catalyst, and further enhance the NH 3 -SCR activity of the catalyst. Moreover, neither CeO 2 nor SiO 2 has biological toxicity, and CeO 2 also exhibits good sulfur resistance potential. Therefore, the cerium-silicon composite oxide combining CeO 2 and SiO 2 may be a potential NH 3 -SCR catalyst with good application prospects.
- the objective of the present invention is to provide a method for preparing a cerium-silicon composite oxide, which has simple raw materials, low cost and simple method.
- Another object of the present invention is to provide a cerium-silicon composite oxide as a flue gas denitration catalyst with better low-temperature activity, high N 2 selectivity, and superior sulfur poisoning resistance, which can be used in flue gas denitration in coal-fired power plants.
- a preparation method of cerium-silicon composite oxide includes the following steps:
- Step 1) Add concentrated ammonia water dropwise to the resulting mixed solution under stirring to cause precipitation and aging precipitation;
- Step 2) The obtained precipitate is filtered, washed, dried and calcined to obtain a cerium-silicon composite oxide.
- the concentration of the cerium ammonium nitrate ethanol solution is 0.005 mol/L to 0.2 mol/L.
- the duration of the continued stirring is 1 h.
- the dropping of concentrated ammonia water is stopped when the pH of the mixed solution is 10, and the concentration of the concentrated ammonia water is 13.2 mol/L.
- the time for the aging precipitation is 12h.
- the washing is 3 times with deionized water, and the drying is drying in an oven at 100° C. for 12 hours.
- the roasting is in a muffle furnace with a temperature of 550°C and a duration of 4 hours.
- the cerium-silicon composite oxide is obtained by the preparation method of the cerium-silicon composite oxide.
- the cerium-silicon composite oxide is Ce-2Si.
- cerium-silicon composite oxide as a flue gas denitration catalyst.
- both cerium ammonium nitrate and TEOS can be dissolved in ethanol, and after adding concentrated ammonia to the solution, both cerium ammonium nitrate and TEOS can be hydrolyzed and precipitated quickly, so the co-precipitation method is adopted to combine the cerium ammonium nitrate and TEOS in After dissolving and mixing uniformly in ethanol, an excessive amount of ammonia is added dropwise to make the precipitation complete, and then the cerium-silicon composite oxide catalyst can be prepared by aging, washing, drying and roasting.
- the method for preparing a cerium-silicon composite oxide provided by the present invention has simple raw materials, low cost, environmentally friendly, simple preparation method, and large-scale production;
- the cerium-silicon composite oxide provided by the present invention has a larger specific surface area, stronger acidity and special surface adsorption mechanism due to the doping of SiO 2 , which effectively improves the CeO 2
- the NH 3 -SCR activity further improves the water and sulfur resistance of the catalyst; as a flue gas denitration catalyst, the cerium-silicon composite oxide has good activity at medium and low temperatures, high N 2 selectivity, superior sulfur poisoning resistance, and environmentally friendly , Has a wide range of industrial application prospects.
- Figure 1 shows the X-ray diffraction (XRD) results of the cerium-silicon composite oxide catalyst and pure CeO 2 ;
- Figure 2 is a graph showing the results of Raman spectra of the cerium-silicon composite oxide catalyst and pure CeO 2 ;
- Figure 3 is the result of the NH 3 -SCR reaction between a cerium-silicon composite oxide catalyst and pure CeO 2 , where (a) is the NO conversion rate and (b) is the N 2 selectivity;
- Figure 4 is a graph showing the test results of the sulfur resistance of the cerium-silicon composite oxide catalyst at 250°C.
- XRD X-ray diffraction
- Raman spectroscopy Raman spectroscopy
- NH 3 -SCR reaction catalytic performance test
- sulfur poisoning performance test sulfur poisoning performance test and other characterization methods to evaluate its bulk structure and catalytic performance
- Fig. 1 The XRD results in Fig. 1 show that within the range of the feed concentration mentioned in the present invention, Ce and Si can be mixed together well, the degree of crystallization of CeO 2 is very low, and SiO 2 reduces the degree of crystallization of CeO 2 .
- the result of Raman in Fig. 2 also shows that the crystal structure of CeO 2 is destroyed, a strong interaction occurs between CeO 2 and SiO 2 and the oxygen defect concentration increases.
- the result of the NH 3 -SCR reaction in Figure 3 shows that the catalytic performance of the cerium-silicon composite oxide catalyst is significantly better than that of CeO 2.
- the NO conversion rate of the cerium-silicon composite oxide is as high as about 90%, and its N 2 selectivity is close to 100%.
- the NO conversion rate of pure CeO 2 is less than 30%, and the N 2 selectivity decreases rapidly as the temperature increases.
- XRD results in Figure 1 show that Ce and Si can be mixed together well within the feeding concentration range mentioned in the present invention.
- the degree of crystallization of CeO 2 is very high. Low, SiO 2 reduces the crystallinity of CeO 2 .
- the result of Raman in Fig. 2 also shows that the crystal structure of CeO 2 is destroyed, a strong interaction occurs between CeO 2 and SiO 2 and the oxygen defect concentration increases.
- the results of the NH 3 -SCR reaction in Figure 3 show that the catalytic performance of the cerium-silicon composite oxide catalyst is significantly better than that of CeO 2.
- the NO conversion rate of the cerium-silicon composite oxide is as high as about 90%, and its N 2 selectivity is close to 100%.
- the NO conversion rate of pure CeO 2 is less than 30%, and the N 2 selectivity decreases rapidly as the temperature increases.
- Figure 4 shows that the cerium-silicon composite oxide exhibits excellent sulfur poisoning resistance at 250°C, and the NO conversion rate has been stable above 90% for a long time without a significant downward trend. However, the NO conversion rate of CeO 2 has dropped seriously, showing Obvious characteristics of sulfur poisoning.
- Example 7 Determination of catalytic performance of cerium-silicon composite oxide for denitration
- the prepared cerium-silicon composite oxide catalyst was applied to the NH 3 -SCR reaction, and the specific reaction conditions were as follows: the catalytic reaction test was carried out in a fixed-bed continuous flow quartz reactor. The particle size of the catalyst is 60-80 mesh, and the dosage is 250 mg.
- the reaction gas composition is: 500 ppm NO, 500 ppm NH 3 , 200 ppm SO 2 , 5% O 2 , and N 2 as the balance gas, and the gas space velocity in the reaction is 30000 mL ⁇ g -1 ⁇ h -1 . Before the reaction, the catalyst needs to be purged with high purity N 2 at 200°C for 1 h.
- the catalytic reaction is carried out at 50-450°C, and the activity data is collected after the reaction reaches equilibrium.
- the product was detected and analyzed by Thermofisher IS10 FTIR, and the NO conversion rate and N 2 selectivity were calculated by the following formula:
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
L'invention concerne un procédé de préparation d'oxyde composite de silicium de cérium et un produit ainsi qu'une application associés. Selon le procédé, du nitrate d'ammonium et de cérium et de l'orthosilicate de tétraéthyle (TEOS) sont mélangés et dissous dans de l'alcool éthylique, puis dans un état d'agitation, de l'eau ammoniacale plus forte est ajoutée goutte à goutte jusqu'à ce que la précipitation soit achevée, puis l'oxyde composite de silicium de cérium est obtenu par vieillissement, filtration, lavage, séchage et calcination. Par rapport au CeO2 pur, l'oxyde composite de silicium de cérium a une surface spécifique plus grande, une acidité plus élevée, et un mécanisme d'adsorption de surface spécial, et l'activité de CeO2 pour catalyser une réaction de NH3-SCR est efficacement améliorée. L'oxyde composite de silicium de cérium sert de catalyseur de dénitration de gaz de combustion, et a une meilleure activité à moyenne et faible température, une sélectivité élevée de N2, une résistance supérieure à l'empoisonnement par le soufre et respecte l'environnement. Le procédé de préparation de l'oxyde composite de silicium de cérium est simple, les matières premières sont simples et faciles à obtenir, et l'oxyde composite de silicium de cérium peut être produit à grande échelle et présente une large perspective d'application industrielle.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910602488.8 | 2019-07-04 | ||
| CN201910602488.8A CN110270321A (zh) | 2019-07-04 | 2019-07-04 | 一种铈硅复合氧化物的制备方法及其产物和应用 |
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| WO2021000458A1 true WO2021000458A1 (fr) | 2021-01-07 |
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| PCT/CN2019/112305 WO2021000458A1 (fr) | 2019-07-04 | 2019-10-21 | Procédé de préparation d'oxyde composite de silicium de cérium et produit ainsi qu'application associés |
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| CN (1) | CN110270321A (fr) |
| WO (1) | WO2021000458A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114774932A (zh) * | 2022-03-15 | 2022-07-22 | 宁波吉海金属科技有限公司 | 一种航空航天不锈钢管道用酸洗钝化剂 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110270321A (zh) * | 2019-07-04 | 2019-09-24 | 南京大学 | 一种铈硅复合氧化物的制备方法及其产物和应用 |
| CN111217377B (zh) * | 2020-02-24 | 2023-02-07 | 宝鸡文理学院 | 铈掺杂介孔氧化硅材料的一步绿色合成方法 |
| CN113000044B (zh) * | 2021-03-15 | 2023-01-24 | 四川大学 | 二氧化碳氧化乙烷脱氢催化剂及其制备方法 |
| CN113209961A (zh) * | 2021-04-13 | 2021-08-06 | 苏州西热节能环保技术有限公司 | 一种高抗硫超宽温结构化改性scr催化剂及制备方法 |
| CN113828130A (zh) * | 2021-10-28 | 2021-12-24 | 辽宁基伊能源科技有限公司 | 基于石墨烯改性碳酸钙脱硝剂的制备方法及其应用 |
| CN114904540A (zh) * | 2022-05-10 | 2022-08-16 | 福州大学 | 一种低温锰基催化剂及其制备方法和应用 |
| CN115518652A (zh) * | 2022-06-13 | 2022-12-27 | 安徽理工大学 | 一种硅铈复合微孔材料封装金属催化剂及其制备方法与应用 |
| CN116371399A (zh) * | 2023-03-28 | 2023-07-04 | 南京大学 | 一种铌改性铈硅混合氧化物催化剂的制备方法及其应用 |
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| US20020090512A1 (en) * | 2000-11-15 | 2002-07-11 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Composite oxide powder, a method for producing the same and a catalyst using the same |
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| CN114774932A (zh) * | 2022-03-15 | 2022-07-22 | 宁波吉海金属科技有限公司 | 一种航空航天不锈钢管道用酸洗钝化剂 |
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